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Water → HCID 86584208, 화합물

HRID 1837412
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HRID 1837412 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[S:11]([CH2:14][S:15]([C:18]([F:21])([F:20])[F:19])(=[O:17])=[O:16])(=[O:13])=[O:12].S([N:32]=[N+:33]=[N-])(C1C=CC(C)=CC=1)(=O)=O.C(N(CC)CC)C.O>C(#N)C.ClCCl>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[S:11]([C:14]([S:15]([C:18]([F:21])([F:19])[F:20])(=[O:16])=[O:17])=[N+:32]=[N-:33])(=[O:13])=[O:12]
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참가 물질

7

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HCID 962WaterHCID 8471TriethylamineHCID 13661p-Toluenesulfonyl azideHCID 22677136HCID 22677136, 화합물

생성물 1

HCID 86584208HCID 86584208, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매
HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

Crude 2-naphthalenesulfonyl-trifluoromethanesulfonyl-methane (5 g, 0.014 mole) is dissolved in acetonitrile (150 ml) under nitrogen and the solution is cooled to 0° C. using an ice bath. Tosyl azide (8.3 g, 0.042 mole) and then triethylamine (3.9 ml, 0.028 mole) are added in one portion and the reaction mixture is stirred at that temperature for 24 h. After adding water (400 ml) and dichloromethane (200 ml), the phases are separated and the aqueous layer is extracted twice with dichloromethane (150 ml) and the combined organic phases are washed with 1 N HCl, saturated sodium bicarbonate and water. After drying over MgSO4 and removal of the solvent, the crude product is obtained as orange oil.

후처리

  1. customthe phases are separated
  2. extractionthe aqueous layer is extracted twice with dichloromethane (150 ml)
  3. washthe combined organic phases are washed with 1 N HCl, saturated sodium bicarbonate and water
  4. dry with materialAfter drying over MgSO4 and removal of the solvent

출처 및 근거

ORD 기록
ord-8f1beb0aaa4f444c93b16c30dd22cacb
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06783912B2

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